CN110887823A - Device and method for measuring iron in water sample by sequential injection-fluorescence method - Google Patents
Device and method for measuring iron in water sample by sequential injection-fluorescence method Download PDFInfo
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Abstract
The invention discloses a device and a method for measuring iron in a water sample by a sequential injection-fluorescence method, which comprises a six-position selector valve, a storage tube, an injection pump, a first two-position three-way valve, a detection pool, a light source, a photoelectric detector, a water pump, a second two-position three-way valve, a water bath sleeve and a plastic box, wherein the injection pump is connected with the six-position selector valve; one end of the storage pipe is connected with the inlet end of the six-position selection valve, and the other end of the storage pipe is connected with the injection pump through the first two-position three-way valve; the detection pool is connected with the six-position selector valve, the light source and the photoelectric detector are respectively connected with the detection pool through optical fibers, the detection pool is arranged in the water bath sleeve, the water inlet of the water pump is connected with the water outlet of the second two-position three-way water valve, the water outlet of the water pump is connected with the water inlet of the water bath sleeve, and two inlet ends of the second two-position three-way valve are respectively connected with the water bath at 70 ℃ and the water bath at 25 ℃. The invention has the beneficial effects that: the combined sequential injection technology and the fluorescence analysis method have the advantages of simple and reliable system hardware, low detection limit, easy realization of automatic control of the processes of mixing, reaction, measurement and the like of the sample and the reagent, and reduction of human intervention.
Description
The technical field is as follows:
the invention belongs to the field of analytical chemistry detection, and particularly relates to a device and a method for determining iron in a water sample by a sequential injection fluorescence method.
Background art:
iron is an essential element for many phytoplankton and microorganism life processes, and plays an important role in respiration, photosynthesis and oxygen transfer in cells. In some waters, iron even limits phytoplankton growth and also limits the uptake of atmospheric CO by phytoplankton2And further affect global climate change. Therefore, the analysis of iron has been receiving great attention.
At present, methods for measuring iron in a water sample mainly comprise spectrophotometry, electrochemical analysis, atomic absorption, fluorescence analysis and the like. Compared with the flow injection technology, the sequential injection technology has the advantages of less reagent consumption, high automation degree and simple hardware, and overcomes the defects of unstable flow injection flow rate and more accurate reagent addition due to the adoption of the injection pump to replace a peristaltic pump.
The invention combines a sequential injection technology and a fluorescence analysis method, and invents a device and a method for measuring the concentration of iron in a water sample (comprising seawater and fresh water). The method can not only reach a very low detection limit (up to 0.3nM), but also realize the determination of the iron concentration in the sample under an acidic condition (pH 1.6-2.0). For a water sample needing to determine the iron concentration, the water sample needs to be acidified to the pH value less than or equal to 2.0 for storage after being collected, and the method can be used for directly determining the iron concentration without regulating the pH value of the sample again (such as to be neutral).
The invention content is as follows:
aiming at the defects in the prior art, the invention provides a device and a method for measuring iron in a water sample by a sequential injection-fluorescence method. An apparatus for determining iron in a water sample by sequential injection-fluorometry, comprising: the device comprises a six-position selector valve, a storage pipe, an injection pump, a first two-position three-way valve, a detection pool, a light source, a photoelectric detector, a water pump, a second two-position three-way valve, a water bath sleeve and a plastic box; one end of the storage pipe is connected with the inlet end of the six-position selector valve, and the other end of the storage pipe is connected with the injection pump through the first two-position three-way valve; the detection pool is connected with a six-position selector valve, a light source and a photoelectric detector are respectively connected with the detection pool through optical fibers, the detection pool is arranged in a water bath sleeve, a water inlet of a water pump is connected with a water outlet of a second two-position three-way water valve, a water outlet of the water pump is connected with a water inlet of the water bath sleeve, two inlet ends of the second two-position three-way valve are respectively connected with water baths at 70 ℃ and 25 ℃, the six-position selector valve has six ports (P1-P6), and the six-position selector valve is respectively connected with a sample, a fluorescent reagent, a surfactant, the detection pool, 0.1M hydrochloric acid and an. The water bath sleeve, the detection pool, the light source and the detector are all arranged in an opaque plastic box.
In one embodiment, the tubing is made of Teflon tubing with an inner diameter of 0.8 mm.
In one embodiment, the detection cell is a glass capillary tube with an inner diameter of 1 mm.
In one embodiment, the optical fiber connected between the light source, the detection cell and the photodetector is a silica optical fiber.
In one embodiment, the light source is a deuterium lamp.
In one embodiment, the photodetector is a photomultiplier tube or a charge coupled device.
A method for determining iron in a water sample by sequential injection-fluorimetry, comprising the steps of:
s1), sequentially sucking the acidified water sample (pH 2.0), the fluorescent reagent and the surfactant into the storage tube (2) through the six-position selector valve (1) by using the syringe pump (3);
s2), injecting the mixed solution in the S1) into a detection pool (5) through a six-position selector valve (1) by a syringe pump (3);
s3) and the detection cell (5) are heated for 15 minutes by a water bath at 70 ℃, and then cooled for 5 minutes by a water bath at 25 ℃, wherein the excitation wavelength of fluorescence analysis is 317nm, and the detection wavelength of the detector is 534nm of emission light intensity.
In one embodiment, the fluorescent reagent is 5- (4-methoxyphenylazo) -8- (4-tolylsulfonamide) quinoline dissolved in ethanol at a concentration of 40-80. mu.M.
In one embodiment, the surfactant is cetyltrimethylammonium bromide dissolved in pure water at a concentration of 6-8 mM.
The invention has the beneficial effects that: the combination of sequential injection technology and fluorescence analysis method has simple and reliable system hardware, easy realization of automatic control of the mixing, reaction, measurement and other processes of the sample and the reagent, and reduction of human intervention. The method can realize the determination of the iron in the water sample under the acidic condition, the sample demand is less (less than 500 mu l), and the detection limit is low (less than or equal to 0.3nM), so the iron in the acidified water sample can be directly determined, and the pH value of the sample is prevented from being adjusted again.
Description of the drawings:
FIG. 1 is a schematic diagram of an apparatus for sequential injection-fluorometric determination of iron in a water sample, according to an embodiment of the present invention.
Wherein the reference numbers in the figures: 1-six-position selector valve, 2-storage tube, 3-injection pump, 4-first two-position three-way valve, 5-detection cell, 6-light source, 7-photoelectric detector, 8-water pump, 9-second two-position three-way valve, 10-water bath sleeve, 11-black plastic box, 12-connecting optical fiber, 13-water bath sleeve water inlet, 14-water bath sleeve water outlet, P1-P6 is six-position selector valve 6 ports.
The specific implementation mode is as follows:
the above and other features, properties and advantages of the present invention will become more apparent from the following description of the embodiments with reference to the accompanying drawings in which like reference numerals denote like features throughout the several views, wherein:
referring to fig. 1, fig. 1 is a schematic diagram illustrating the operation of an apparatus for measuring iron in a water sample by sequential injection-fluorometry according to an embodiment of the present invention. In this embodiment, the device is composed of a six-position selector valve 1, a storage tube 2, an injection pump 3, a first two-position three-way valve 4, a detection pool 5, a light source-deuterium lamp 6, a photoelectric detector 7, a water pump 8, a second two-position three-way valve 9, a water bath sleeve 10 and a black plastic box 11. One end of a storage pipe 2 is connected with a six-position selector valve 1, the other end of the storage pipe is connected with an injection pump 3 through a first two-position three-way valve 4, a detection pool 5 is connected with the six-position selector valve 1, a light source 6 and a photoelectric detector 7 are respectively connected with the detection pool 5 through quartz optical fibers 12, the detection pool 5 is arranged in a water bath sleeve 10, a water inlet of a water pump 8 is connected with a water outlet of a second two-position three-way valve 9, the water outlet of the water pump 8 is connected with a water inlet of the water bath sleeve 10, two water inlets of the second two-position three-way valve 9 are respectively connected with a 70 ℃ water bath and a 25 ℃ water bath, and six ports of the six-position selector valve 1 are respectively connected with a sample, a fluorescent reagent. The water bath sleeve 10, the detection cell 5, the light source 6 and the photoelectric detector 7 are all arranged in an opaque plastic box 11.
Preferably, the photodetector 7 is a photomultiplier tube or a charge coupled device.
Preferably, the fluorescent reagent is 5- (4-methoxyphenylazo) -8- (4-tolylsulfonamide) quinoline ethanol solution, and the concentration is 40-80 mu M.
Preferably, the surfactant is hexadecyl trimethyl ammonium bromide dissolved in pure water, and the concentration of the surfactant is 6-8 mM.
The following are two specific examples given by the inventors, but not limited to these two examples.
The first embodiment: determination of iron in acidified preserved water sample
The main determination steps are as follows:
1. a six-position selection valve (1) is arranged at a P1 port, and a syringe pump (3) is used for pumping 400 mu l of sample;
2. a six-position selection valve (1) is arranged at a P2 port, and a syringe pump (3) is used for pumping 200 mu l of fluorescent reagent;
3. a six-position selection valve (1) is arranged at a P3 port, and a syringe pump (3) is used for pumping 200 mu l of surfactant;
4. a six-position selection valve (1) is arranged at a P4 port, and a syringe pump (3) is pushed reversely to inject the mixed solution into the detection cell;
5. the second two-position three-way valve (9) is connected with a 70 ℃ water bath, the water pump (8) is opened, the water is kept for 15 minutes, and the water pump (8) is closed;
6. the second two-position three-way valve (9) is connected with a water bath at 25 ℃, a water pump (8) is opened, the water bath is kept for 5 minutes, and the water pump (8) is closed;
7. opening a light source passage (the light source (6) is started for more than 30 minutes in advance), and detecting the fluorescence signal intensity by the photoelectric detector (7);
8. ultrapure water is sucked by a syringe pump (3), and all pipelines are cleaned in sequence.
Second embodiment: determination of iron in raw water sample (non-acidified water sample)
The main determination steps are as follows:
1. a six-position selection valve (1) is arranged at a P1 port, and a syringe pump (3) is used for pumping 360 mu l of sample;
2. a six-position selection valve (1) is arranged at a P5 port, and a syringe pump (3) is used for pumping 40 mu l of 0.1M hydrochloric acid;
3. a six-position selection valve (1) is arranged at a P2 port, and a syringe pump (3) is used for pumping 200 mu l of fluorescent reagent;
4. a six-position selection valve (1) is arranged at a P3 port, and a syringe pump (3) is used for pumping 200 mu l of surfactant;
5. a six-position selection valve (1) is arranged at a P4 port, and a syringe pump (3) is pushed reversely to inject the mixed solution into the detection cell;
6. the second two-position three-way valve (9) is connected with a 70 ℃ water bath, the water pump (8) is opened, the water is kept for 15 minutes, and the water pump (8) is closed;
7. the second two-position three-way valve (9) is connected with a water bath at 25 ℃, a water pump (8) is opened, the water bath is kept for 5 minutes, and the water pump (8) is closed;
8. opening a light source passage (the light source (6) is started for more than 30 minutes in advance), and detecting the fluorescence signal intensity by the photoelectric detector (7);
9. ultrapure water is sucked by a syringe pump (3), and all pipelines are cleaned in sequence.
The present invention and its embodiments have been described above schematically, without limitation, and what is shown in the drawings is only one of the embodiments of the present invention, and the actual structure is not limited thereto. Therefore, if the person skilled in the art receives the teaching, without departing from the spirit of the invention, the person skilled in the art shall not inventively design the similar structural modes and embodiments to the technical solution, but shall fall within the scope of the invention.
Claims (9)
1. An apparatus for determining iron in a water sample by sequential injection-fluorometry, comprising: the device comprises a six-position selector valve (1), a storage pipe (2), an injection pump (3), a first two-position three-way valve (4), a detection pool (5), a light source (6), a photoelectric detector (7), a water pump (8), a second two-position three-way valve (9), a water bath sleeve (10), a plastic box (11) and an optical fiber (12); wherein the content of the first and second substances,
one end of the storage pipe (2) is connected with the inlet end (1) of the six-position selector valve, and the other end of the storage pipe (2) is connected with the injection pump (3) through a first two-position three-way valve (4);
the detection pool (5) is connected with the six-position selector valve (1), the light source (6) and the photoelectric detector (7) are respectively connected with the detection pool (5) through optical fibers (12), the detection pool (5) is arranged in a water bath sleeve (10), a water inlet of the water pump (8) is connected with a water outlet of a second two-position three-way water valve (9), a water outlet of the water pump (8) is connected with a water inlet (13) of the water bath sleeve, two inlet ends of the second two-position three-way valve (9) are respectively connected with water baths at 70 ℃ and 25 ℃, the six-position selector valve (1) has six ports (P1-P6), and a sample, a fluorescent reagent, a surfactant, the detection pool, 0.1M hydrochloric acid and an iron standard solution are respectively connected through pipelines. The water bath sleeve (10), the detection pool (5), the light source (6) and the detector (7) are all arranged in an opaque plastic box (11).
2. The device for determining iron in a water sample by a sequential injection-fluorescence method according to claim 1, wherein: the pipeline is made of polytetrafluoroethylene tubes, and the inner diameter of the pipeline is 0.8 mm.
3. The device for determining iron in a water sample by a sequential injection-fluorescence method according to claim 1, wherein: the detection cell (5) is a glass capillary tube with the inner diameter of 1 mm.
4. The device for determining iron in a water sample by a sequential injection-fluorescence method according to claim 1, wherein: the optical fiber (12) connected among the light source (6), the detection cell (5) and the photoelectric detector (7) is a quartz optical fiber.
5. The device for determining iron in a water sample by a sequential injection-fluorescence method according to claim 1, wherein: the light source (6) is a deuterium lamp.
6. The device for determining iron in a water sample by a sequential injection-fluorescence method according to claim 1, wherein: the photodetector (7) is a photomultiplier or a charge coupled device.
7. A method for determining iron in a water sample by a sequential injection-fluorescence method, which is characterized by comprising the following steps: the method comprises the following steps:
s1), sequentially sucking the acidified water sample (pH 2.0), the fluorescent reagent and the surfactant into the storage tube (2) through the six-position selector valve (1) by using the syringe pump (3);
s2), injecting the mixed solution in the S1) into a detection pool (5) through a six-position selector valve (1) by a syringe pump (3);
s3) and the detection cell (5) are heated for 15 minutes by a water bath at 70 ℃, and then cooled for 5 minutes by a water bath at 25 ℃, wherein the excitation wavelength of fluorescence analysis is 317nm, and the detection wavelength of the detector is 534nm of emission light intensity.
8. The method for determining iron in an aqueous sample by sequential injection-fluorometry according to claim 7, wherein: the fluorescent reagent is a solution formed by dissolving 5- (4-methoxyphenylazo) -8- (4-tolylsulfonamide) quinoline in ethanol, and the concentration of the fluorescent reagent is 40-80 mu M.
9. The method for determining iron in an aqueous sample by sequential injection-fluorometry according to claim 7, wherein: the surfactant is hexadecyl trimethyl ammonium bromide dissolved in pure water, and the concentration of the surfactant is 6-8 mM.
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| CN201911155932.2A CN110887823A (en) | 2019-11-22 | 2019-11-22 | Device and method for measuring iron in water sample by sequential injection-fluorescence method |
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Application publication date: 20200317 |